CN109647201A - The method of ultrasonic wave added interfacial polymerization continuous production External Pressure Type hollow fiber nanofiltration membrane - Google Patents
The method of ultrasonic wave added interfacial polymerization continuous production External Pressure Type hollow fiber nanofiltration membrane Download PDFInfo
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- CN109647201A CN109647201A CN201811572235.2A CN201811572235A CN109647201A CN 109647201 A CN109647201 A CN 109647201A CN 201811572235 A CN201811572235 A CN 201811572235A CN 109647201 A CN109647201 A CN 109647201A
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- hollow fiber
- nanofiltration membrane
- continuous production
- external pressure
- pressure type
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/02—Reverse osmosis; Hyperfiltration ; Nanofiltration
- B01D61/027—Nanofiltration
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D63/00—Apparatus in general for separation processes using semi-permeable membranes
- B01D63/02—Hollow fibre modules
- B01D63/021—Manufacturing thereof
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0002—Organic membrane manufacture
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/08—Hollow fibre membranes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/30—Polyalkenyl halides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/30—Polyalkenyl halides
- B01D71/32—Polyalkenyl halides containing fluorine atoms
- B01D71/34—Polyvinylidene fluoride
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/40—Polymers of unsaturated acids or derivatives thereof, e.g. salts, amides, imides, nitriles, anhydrides, esters
- B01D71/42—Polymers of nitriles, e.g. polyacrylonitrile
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/66—Polymers having sulfur in the main chain, with or without nitrogen, oxygen or carbon only
- B01D71/68—Polysulfones; Polyethersulfones
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Water Supply & Treatment (AREA)
- Manufacturing & Machinery (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention belongs to nanofiltration field of membrane preparation, more particularly to a kind of method of ultrasonic wave added interfacial polymerization continuous production External Pressure Type hollow fiber nanofiltration membrane, include the following steps: Hollow Fiber Ultrafiltration basement membrane being immersed in ultrasonic vibration 1-2s in water phase, after taking-up is dried, it is immersed in 10-60s in organic phase again, taking-up, which is placed in 80-130 DEG C of baking oven, carries out heat treatment 0.5-10min to get required product；Wherein the water phase includes polyamine, proton absorbent and water；The organic phase includes polynary acyl chlorides and n-hexane.The concentration of the polyamine is 1-3% (w/w), and the concentration of proton absorbent is 0.5-5% (w/w)；Water phase infiltrating time can be shortened 80% during serialization prepares hollow fiber nanofiltration membrane by this technology, while not influence film wire performance, and the cost of hollow fiber nanofiltration membrane serialization spinning is greatly reduced, improves production efficiency.
Description
Technical field
The invention belongs to nanofiltration field of membrane preparation, and in particular to a kind of ultrasonic wave added interfacial polymerization continuous production External Pressure Type
The method of hollow fiber nanofiltration membrane.
Background technique
During serialization spins External Pressure Type hollow fiber nanofiltration membrane, due to being limited by device length, place etc., interface
Polymerization water phase infiltrating time is restricted, and causes water phase infiltration insufficient, and obtained nanofiltration membrane water yield, salt rejection rate produces water difference
Degree decline.
Summary of the invention
During overcoming continuous production hollow fiber nanofiltration membrane, due to infiltrating insufficient cause
The problem of film properties decline, provides a kind of side of ultrasonic wave added interfacial polymerization continuous production External Pressure Type hollow fiber nanofiltration membrane
Method.
The present invention to achieve the above object, using following technical scheme:
A kind of method of ultrasonic wave added interfacial polymerization continuous production External Pressure Type hollow fiber nanofiltration membrane, including following steps
It is rapid:
Ultrafiltration membranes are immersed in water phase ultrasonic vibration 1-10s, it is preferred that ultrafiltration membranes are immersed in water phase ultrasonic vibration
1-2s；After taking-up is dried, then it is immersed in 10-60s in organic phase, taking-up, which is placed in 80-130 DEG C of baking oven, to be heat-treated
0.5-10min is to get required product；
Wherein the water phase includes polyamine, proton absorbent and water；The organic phase include polynary acyl chlorides with
And n-hexane.
The ultrafiltration membranes are one of polysulfones, polyether sulfone, Kynoar, polyacrylonitrile, polyvinyl chloride.
The proton absorbent is organic base or inorganic base.The proton absorbent be sodium hydroxide, sodium phosphate,
Triethylamine, the mixing of one or more of 4-dimethylaminopyridine.
The concentration of the polyamine is 1-3% (w/w), and the concentration of proton absorbent is 0.5-5% (w/w)；
The concentration of the polynary acyl chlorides is 0.05~0.2% (w/w).
Compared with prior art, the beneficial effects of the present invention are:
The present invention is the key technology of continuous production External Pressure Type hollow fiber nanofiltration membrane.All the time, with serialization
Mode produces the great difficult problem that hollow fiber nanofiltration membrane is technical field of membrane, and this is the key that one step of doughnut industrialization.
And during continuous production, due to being influenced by practical factors such as equipment, places, the key parameter in preparation process is not
It is able to satisfy requirement, therefore develops series of key techniques to realize the continuous production of External Pressure Type doughnut.Even if the present invention its
One of: during serialization prepares hollow fiber nanofiltration membrane, using ultrasonic assisted technique, water phase infiltrating time can be shortened
80%, while film wire performance is not influenced, the cost of hollow fiber nanofiltration membrane serialization spinning is greatly reduced, improves production efficiency.
Specific embodiment
In order to make those skilled in the art more fully understand technical solution of the present invention, below with reference to embodiment pair
The present invention is described in further detail.
A kind of method of ultrasonic wave added interfacial polymerization continuous production External Pressure Type hollow fiber nanofiltration membrane, including following steps
It is rapid:
Hollow Fiber Ultrafiltration basement membrane is immersed in water phase ultrasonic vibration 1-10s, (ultrasonic transducer is placed in immediately below film wire,
It similarly hereinafter) takes out after drying, then is immersed in 10-60s in organic phase, taking-up, which is placed in 80-130 DEG C of baking oven, to be heat-treated
0.5-10mins is to get required product；Wherein the water phase includes polyamine, proton absorbent and water；Described is organic
It mutually include polynary acyl chlorides and n-hexane.
The Hollow Fiber Ultrafiltration basement membrane is polysulfones, in polyether sulfone, Kynoar, polyacrylonitrile, polyvinyl chloride
It is a kind of.The proton absorbent is organic base or inorganic base.
The concentration of the polyamine is 1-3% (w/w), and the concentration of proton absorbent is 0.5-5% (w/w)；
The concentration of the polynary acyl chlorides is 0.05~0.2% (w/w).
Embodiment 1:
Water phase: 2g piperazine (organic amine), 0.5g triethylamine (proton absorbent), 100g deionized water.
Organic phase: 0.1g pyromellitic trimethylsilyl chloride (polynary acyl chlorides), 100g n-hexane (organic solvent).
Interfacial polymerization process: ultrafiltration membranes are immersed in water phase ultrasonic vibration 1s, take out naturally dry 10min.Again by it
Submergence and 10s in organic phase.After taking out 1min, it is put into 30s in 80 DEG C of baking ovens and is immersed in get hollow fiber nanofiltration membrane product
It is to be measured in deionized water.
Embodiment 2:
Water phase: 2g piperazine, 0.1gNaOH (proton absorbent), 100g deionized water.
Organic phase: 0.1g pyromellitic trimethylsilyl chloride, 100g n-hexane.
Interfacial polymerization process: ultrafiltration membranes are immersed in water phase ultrasonic vibration 1s, take out naturally dry 10min.Again by it
Submergence and 10s in organic phase.After taking out 1min, it is put into 30s in 80 DEG C of baking ovens and is immersed in get hollow fiber nanofiltration membrane product
It is to be measured in deionized water.
Embodiment 3:
A phase: 2g piperazine, 0.5g triethylamine, 100 parts of deionized waters.
B phase: 0.1g pyromellitic trimethylsilyl chloride, 100g n-hexane.
Interfacial polymerization process: ultrafiltration membranes are immersed in water phase ultrasonic vibration 2s, take out naturally dry 10min.Again by it
Submergence and 10s in organic phase.After taking out 1min, it is put into 30s in 80 DEG C of baking ovens and is immersed in get hollow fiber nanofiltration membrane product
It is to be measured in deionized water.
Embodiment 4: embodiment 4 is same as Example 1, and difference is only that, it is super that Hollow Fiber Ultrafiltration basement membrane is immersed in water phase
10s is swung in acoustic shock.
Comparative example 1: comparative example 1 is same as Example 1, and ultrafiltration membranes are immersed in water phase 2s.
Comparative example 2: comparative example 2 is same as Example 1, and ultrafiltration membranes are immersed in water phase 10s.
Nano filter membrane separating property test method.
Test fluid: being respectively adopted 2000mg/L sodium chloride (NaCl) solution and 2000mg/L magnesium sulfate (MgSO4) solution is surveyed
Examination.
Operating parameter: it is tested using nanofiltration membrane evaluation instrument, pressure 0.5MPa, 25 DEG C, pH=7.0, the rate of recovery 15%.
Calculation formula:
Rejection R=(CI-CO)/CI*100%, wherein CI is water inlet conductance, and CO is water outlet conductance；
Flux F=V/ (A*T), wherein V is to produce water volume, and A is membrane area, and T is time of measuring.
Table 1 is nano filter membrane separating property comparison；
Table 1
| Flux (LMH) | NaCl (%) | MgSO4(%) | |
| Embodiment 1 | 38 | 31 | 81 |
| Embodiment 2 | 36 | 37 | 84 |
| Embodiment 3 | 45 | 32 | 85 |
| Embodiment 4 | 37 | 35 | 86 |
| Comparative example 1 | 31 | 27 | 78 |
| Comparative example 2 | 43 | 36 | 84 |
Conclusion: promote diffusion 1-2s (embodiment 1-3) of the water phase to doughnut basement membrane using ultrasonic transducer, film can be made
Silk performance, which reaches, infiltrates 10s (comparative example 2) comparable index with without using ultrasound.
The above is only a preferred embodiment of the present invention, for those of ordinary skill in the art, according to the present invention
Thought, there will be changes in the specific implementation manner and application range, and the content of the present specification should not be construed as to the present invention
Limitation.
Claims (7)
1. a kind of method of ultrasonic wave added interfacial polymerization continuous production External Pressure Type hollow fiber nanofiltration membrane, which is characterized in that packet
Include following step:
Hollow Fiber Ultrafiltration basement membrane is immersed in water phase ultrasonic vibration 1-10s, after taking-up is dried, then is immersed in 10- in organic phase
60s, taking-up, which is placed in 80-100 DEG C of baking oven, carries out heat treatment 0.5-10min to get required product；
Wherein the water phase includes polyamine, proton absorbent and water；The organic phase includes polynary acyl chlorides and just
Hexane.
2. the side of ultrasonic wave added interfacial polymerization continuous production External Pressure Type hollow fiber nanofiltration membrane according to claim 1
Method, which is characterized in that the ultrafiltration membranes are polysulfones, polyether sulfone, Kynoar, polyacrylonitrile, one in polyvinyl chloride
Kind.
3. the side of ultrasonic wave added interfacial polymerization continuous production External Pressure Type hollow fiber nanofiltration membrane according to claim 1
Method, which is characterized in that Hollow Fiber Ultrafiltration basement membrane is immersed in the water phase ultrasonic vibration time as 1-2s.
4. the side of ultrasonic wave added interfacial polymerization continuous production External Pressure Type hollow fiber nanofiltration membrane according to claim 1
Method, which is characterized in that the proton absorbent is organic base or inorganic base.
5. the side of ultrasonic wave added interfacial polymerization continuous production External Pressure Type hollow fiber nanofiltration membrane according to claim 1
Method, which is characterized in that the proton absorbent is sodium hydroxide, sodium phosphate, triethylamine, one of 4-dimethylaminopyridine
Or a variety of mixing.
6. the side of ultrasonic wave added interfacial polymerization continuous production External Pressure Type hollow fiber nanofiltration membrane according to claim 1
Method, which is characterized in that the concentration of the polyamine is 1-3% (w/w), and the concentration of proton absorbent is 0.5-5% (w/w).
7. the side of ultrasonic wave added interfacial polymerization continuous production External Pressure Type hollow fiber nanofiltration membrane according to claim 1
Method, which is characterized in that the concentration of the polynary acyl chlorides is 0.05-0.2% (w/w).
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20030076013A (en) * | 2002-03-22 | 2003-09-26 | 주식회사 효성 | Nanofiltration composite membrane and the process for the preparing the same |
| CN101384376A (en) * | 2006-02-15 | 2009-03-11 | 东亚合成株式会社 | Method for producing functional membrane |
| CN103768963A (en) * | 2014-01-23 | 2014-05-07 | 南通苏通分离工程科技有限公司 | Preparation method for polyamide composite nanofiltration membrane |
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2018
- 2018-12-21 CN CN201811572235.2A patent/CN109647201A/en not_active Withdrawn
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20030076013A (en) * | 2002-03-22 | 2003-09-26 | 주식회사 효성 | Nanofiltration composite membrane and the process for the preparing the same |
| CN101384376A (en) * | 2006-02-15 | 2009-03-11 | 东亚合成株式会社 | Method for producing functional membrane |
| CN103768963A (en) * | 2014-01-23 | 2014-05-07 | 南通苏通分离工程科技有限公司 | Preparation method for polyamide composite nanofiltration membrane |
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Application publication date: 20190419 |